Sparanalys av ett Similiaemne foer VX i Blod och Vaevnad med Fastfas-Extraktion och Gasktromatografisk analys med Fosforspecifik Detektion (Trace Analysis of a VX Simulant in Blood and Tissue Samples by Solid Phase Extraction and Gas Chromatographic Analy

摘要

An analytical method for phosphonoacetate, LT-8 in biological samples was developed. It is based on solid phase extraction and analysis by means of gas chromatography and detection with a detector specific for phosphorus (GC/NPD). Selection of column for separation and the condition of the detector were found to be crucial parameters. The method is linear within the field .01-1 micrograms/ml serum. The detection limit for LT-8 is .002 micrograms/ml serum. The reproducibility of the method is about 10% relative standard deviation within the interval .01-1 micrograms/ml serum. The recovery of the extraction procedure is about 75%, when LT-8 is extracted from whole blood. The losses are probably obtained mainly during the separation of blood corpuscles from serum by centrifugation in order to ease the subsequent steps of the sample preparation procedure. The recovery after extraction of .5 micrograms/ml LT-8 added to serum/buffer mixture was 90%. Recovery of LT-8, 2 micrograms/g wet tissue, added to other pig tissue samples (skin and muscle tissues) before the extraction procedure varied from 20-60%. The explanation of this variation is at present not clear and has to be examined further in order to improve the recovery. When standard solutions of LT-8 were analyzed by means of GC/NPD, a relative standard deviation of 1.5% was obtained. When standard solution of LT-8 in ethyl acetate together with the internal standard tributylophosphate (TBP) in the amounts 1-1000 pg were analyzed, the linear regression of the data had a correlation coefficient of .99997. The corresponding correlation coefficient of data from serum samples with LT-8 added was .9978.